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机构地区:[1]天津医科大学肿瘤医院分子影像及核医学诊疗科,国家肿瘤临床医学研究中心,天津市"肿瘤防治"重点实验室,天津300060
出 处:《天津中医药》2014年第4期238-240,共3页Tianjin Journal of Traditional Chinese Medicine
基 金:国家自然科学基金资助项目(30872954);天津市卫生局科技基金资助项目(2012KZ064)
摘 要:【目的】建立超高效液相色谱法同时测定13批不同产地大黄中大黄素、大黄酚、大黄酸、大黄素甲醚、芦荟大黄素等5种游离蒽醌的含量。【方法】采用WatersBEHC18(2.1mm×150mm,1.8μm),以乙腈(A)-0.1%甲酸水溶液(B)为流动相,梯度洗脱[0—3min,19%-+25%A,3-10min,25%--100%A],流速0.3mL/min,柱温30℃,检测波长254nm。【结果】大黄酸、大黄酚、大黄素、大黄素甲醚、芦荟大黄素分别在1.61~80.30,4.98~249.20,3.27-163.30,9.65~482.50,1.67~83.30μg/mL范围内呈现良好的线性关系,平均回收率分别为99.7%,100.4%,100.1%,98.9%,100.9%。相对标准偏差(RSD)分别为1.5%,0.6%,0.8%,0.4%,1.7%。【结论】该方法简便可行,重复性良好,可用于大黄药材的质量控制。[Objective] To develop a UPLC method for simultaneous determination of five anthraquinones (Rhein, Chrysophanol, Emodin, Physcion and Aloe-emodin) in Radix et Rhizom a Rhei from different habitats. [Methods] The analysis was performed on Waters BEH C18 column (2.1 mm×150 mm, 1.8 μm) with a gradient mobile phase of acetonitrile (A)-0.1% Formic acid solution (B)(0N3 min, 19%→25% A, 3-10 min, 25%→100%A) at flow rate of 0.3 mL/min. The column was maintain at 30℃ and the detection wavelength was set at 254 nm. [Results] The linear ranges were 1.61 -80.30 μg/mL for Rhein, 4.98 N249.20 μg/mL for Chrysophanol, 3.27-163.30 μg/mL for Emodin, 9.65 -482.50 μg/mL for Physcion and 1.67-83.30 μg/mL for Aloe-emodin. The average recoveries of the five compounds were 99.7%, 100.4%, 100.1%, 98.9%, 100.9% and RSD were 1.5%, 0.6%, 0.8%, 0.4%, 1.7% respectively. [Conclusion] The rapid and accurate UPLC method was established. This method can be used to assess the quality of Rhubarb.
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